Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Nitric Acid | HCID 944 | — |
| Reactant | Phosphoric Acid | HCID 1004 | — |
| Reactant | Acetylacetone | HCID 31261 | — |
| Reactant | 2-(1-Methylethoxy)benzenamine | HCID 34436 | — |
| Reactant | Potassium Acetate | HCID 517044 | — |
| Reactant | Sodium Nitrite | HCID 23668193 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178468322 | HCID 178468322 | 30.5% |
Reaction Steps
2-(1-Methylethoxy)aniline (1.00 g, 6.62 mmol) was added to a solution of 6 mL of phosphoric acid (85%) and 4 mL of nitric acid (65%) at −6° C., followed by sodium nitrite (0.55 g, 7.95 mmol) in 2 mL of water dropwise at 0° C., and the mixture was stirred at 0° C. for 30 min. Then, to the reaction mixture was added dropwise a solution of potassium acetate (1.95 g, 19.86 mmol) and acetylacetone (0.86 g, 8.61 mmol) in 40 mL of ethanol and 10 mL of water. The mixture was stirred at room temperature overnight, filtered, washed with water, EtOH/H2O (1/1) and hexane, and dried to give the title compound (0.53 g, 30% yield): 1H NMR (400 MHz, CDCl3): δ ppm 1.28-1.41 (6H, m), 2.50 (3H, s), 2.63 (3H, s), 4.53-4.59 (1H, m), 7.21-7.25 (1H, m), 7.62-7.66 (2H, m), 7.77-7.79 (1H, m), 15.01 (1H, s).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08354411B2 |
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| Source dataset | uspto-grants-2013_01 |
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| ORD ID | ord-f04c4140e5384dcfbbe430798578fdaa |
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| Source note | uspto-grants-2013_01 |
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